Nanoparticles of La2CuO4 (LCO) with different particles and crystallite size have been synthesized by the sol-gel method. The samples have been sintered at 600, 650, and 700°C. The sintering process have been performed in atmospheric pressure and vacuum pressure. The structural and morphological properties of the samples have been investigated by the X-Ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Transmission Electron Microscope (TEM). The XRD patterns of the samples have shown that all samples crystallize in orthorhombic structure with Bmab space group. Additionally, Rietveld refinement process have shown that higher sintering temperature, as well sintering process under vacuum pressure, can improve both phase purity and the crystallinity of the samples. SEM and TEM results have also shown that higher sintering temperature results in a sample with larger particle size.